CN110527202A - 具有固化后密封剂层的充气轮胎 - Google Patents

具有固化后密封剂层的充气轮胎 Download PDF

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CN110527202A
CN110527202A CN201910439871.6A CN201910439871A CN110527202A CN 110527202 A CN110527202 A CN 110527202A CN 201910439871 A CN201910439871 A CN 201910439871A CN 110527202 A CN110527202 A CN 110527202A
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ester
rubber
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A.弗兰岑
F.恩祖卢
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Goodyear Tire and Rubber Co
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Abstract

本发明公开了具有固化后密封剂层的充气轮胎。本发明涉及一种制造充气轮胎的方法，包括以下步骤：混合包含弹性体、填料、稀释剂、醌型固化剂、氧化剂型共固化剂；和式1的固化改性剂的密封剂组合物：其中R1和R2独立地为H或C1至C4烷基，或者R1和R2连接在一起形成取代或未取代的亚苯基基团；R3和R4独立地为H、‑OH、‑NH2、C1至C4烷基或‑OR5，其中R5为C1至C4烷基，条件是当R1和R2连接在一起形成取代或未取代的亚苯基基团时，R5为C1至C3烷基；将该密封剂组合物施加到固化轮胎的内表面上；并固化该密封剂组合物。

Description

具有固化后密封剂层的充气轮胎
技术领域
本发明涉及充气轮胎，更具体地涉及具有固化后密封剂层的充气轮胎。
背景技术
已经提出了用于充气轮胎的各种方法、密封剂和轮胎构造，涉及使用液体密封剂涂料，其中密封剂流入穿孔。然而，此类液体密封剂可能在高温下过度流动并导致轮胎失去平衡。而且，液体密封剂在从夏季延续到冬季条件的宽温度范围内可能并不完全可操作或有效。将硫化橡胶材料中的液体密封剂包覆的更复杂的轮胎结构制造起来可能会很昂贵，并且由于轮胎中所需的额外重量也可能产生平衡和悬挂问题。
还已经进一步提出了防刺穿轮胎，其中在未硫化轮胎层之间组装例如可降解丁基橡胶的密封剂层以提供内装式密封剂。通过在两个或更多个非降解的橡胶层（例如，轮胎内衬和轮胎胎体）之间层压密封剂层，该密封剂层在其中对轮胎施加高压的硫化操作期间保持其结构完整性，否则将从其所需的位置处置换降解的橡胶层。然而，通常用于内装式密封剂的胶料（例如有机过氧化物解聚的丁基橡胶）可在较高温度下产生气体，例如在轮胎固化期间或在轮胎使用期间，这可能导致在美学上无吸引力的内衬气泡形成。除了无吸引力之外，这样的气泡形成还可能使密封剂不利地迁移离开其预期位置。为了防止气泡形成，例如可以以增加的厚度提供内衬，但是这会增加构建轮胎的成本。
还已知在固化过程之后或固化后将密封剂层直接施加到轮胎上。此类密封剂层通常粘附地固定到最内部的内衬的暴露表面上，并且可以是粘性和凝胶状的。本领域中已知的此类固化后密封剂可能无法提供足够的针对刺穿物体（如钉子等）的长期密封。
因此，需要改进的用于轮胎的固化后密封剂层。
发明内容
本发明涉及一种制造充气轮胎的方法，包括以下步骤：混合包含弹性体、填料、稀释剂、醌型固化剂、氧化剂型共固化剂（oxidant co-curative）；和式1的固化活化剂的密封剂组合物：
其中R1和R2独立地为H或C1 至C4烷基，或者R1 和R2连接在一起形成取代或未取代的亚苯基基团；R3 和R4 独立地为H、-OH、-NH2、C1 至C4烷基或-OR5，其中R5为C1 至C4烷基，条件是当R1 和R2连接在一起形成取代或未取代的亚苯基基团时，R5为C1 至C3烷基；将该密封剂组合物施加到固化轮胎的内表面上；并固化该密封剂组合物。
本发明公开了以下实施方案：
方案1. 制造充气轮胎的方法，其特征在于包括以下步骤：
混合包含弹性体、填料、稀释剂、醌型固化剂、氧化剂型共固化剂；和式1的固化改性剂的密封剂组合物：
其中R1和R2独立地为H或C1 至C4烷基，或者R1 和R2连接在一起形成取代或未取代的亚苯基基团；R3 和R4 独立地为H、-OH、-NH2、C1 至C4烷基或-OR5，其中R5为C1 至C4烷基，条件是当R1 和R2连接在一起形成取代或未取代的亚苯基基团时，R5为C1 至C3烷基；将所述密封剂组合物施加到固化轮胎的内表面上；并固化所述密封剂组合物。
方案2. 根据方案1的方法，其特征在于所述固化改性剂选自邻苯二甲酸、邻苯二甲酸单烷基酯、邻苯二甲酸二烷基酯、邻苯二甲酸单酰胺、邻苯二甲酸二酰胺、邻苯二甲醛和邻二乙酰苯。
方案3. 根据方案1的方法，其特征在于所述固化改性剂选自邻苯二甲酸二甲酯、邻苯二甲酸二乙酯和邻苯二甲酸二丙酯。
方案4. 根据方案1的方法，其特征在于所述固化改性剂选自马来酸、马来酸单烷基酯、马来酸二烷基酯、马来酸单酰胺、马来酸二酰胺、柠康酸、柠康酸单烷基酯、柠康酸二烷基酯、柠康酸单酰胺、柠康酸二酰胺和2-丁烯二醛-2Z 。
方案5. 根据方案1的方法，其特征在于所述固化改性剂选自马来酸二甲酯、马来酸二乙酯、马来酸二丙酯和马来酸二丁酯。
方案6. 根据方案1的方法，其特征在于所述固化改性剂选自偏苯三甲酸、偏苯三甲酸单烷基酯、偏苯三甲酸二烷基酯、偏苯三甲酸三烷基酯、连苯三甲酸、连苯三甲酸单烷基酯、连苯三甲酸二烷基酯、连苯三甲酸三烷基酯、均苯四甲酸、均苯四甲酸单烷基酯、均苯四甲酸二烷基酯、均苯四甲酸三烷基酯和均苯四甲酸四烷基酯。
方案7. 根据方案1的方法，其特征在于所述密封剂组合物进一步包含选自乙二醇、烷基取代的乙二醇、乙二胺和烷基取代的乙二胺的固化迟延剂。
方案8. 根据方案1的方法，其特征在于所述弹性体选自丁基橡胶、卤化丁基橡胶、EPDM、苯乙烯-丁二烯橡胶、丙烯腈-丁二烯橡胶、丙烯腈-丁二烯-苯乙烯橡胶、聚丁二烯、天然橡胶和合成聚异戊二烯。
方案9. 根据方案1的方法，其特征在于所述氧化剂型共固化剂选自二芳酰基过氧化物、二酰基过氧化物和过氧化酯。
方案10. 根据方案1的方法，其特征在于所述醌型选自苯醌二肟、对对二苯甲酰醌二肟和二苯甲酰对醌二肟。
方案11. 根据方案1的方法，其特征在于所述氧化剂型共固化剂是过氧化苯甲酰。
方案12. 根据方案1的方法，其特征在于所述稀释剂是数均分子量Mn为200至5,000的低分子量弹性体。
方案13. 根据方案1的方法，其特征在于所述密封剂进一步包含油和树脂中的至少一种。
方案14. 根据方案1的方法，其特征在于所述稀释剂是聚异丁烯。
方案15. 根据方案1的方法，其特征在于所述密封剂组合物进一步包含1至10 phr的金属氧化物，所述金属氧化物选自氧化锌、氧化镁和氧化钙。
方案16. 根据方案1的方法，其特征在于混合的步骤包括以下步骤：
将氧化剂型共固化剂与一部分稀释剂组合以形成组分A；
将剩余的成分组合以形成组分B；和
将组分A与组分B混合以形成所述密封剂组合物。
方案17. 充气轮胎，其特征在于通过方案1的方法制造。
附图说明
图1显示了充气轮胎的横截面图，该充气轮胎包含周向密封剂层，其包含粘附在内衬上的轮胎固化后施加的密封剂层。
图2显示了具有轮胎固化后施加的密封剂层的轮胎的一部分的局部横截面图。
图3显示了包含各种固化改性剂的密封剂组合物的固化行为。
具体实施方式
公开了一种制造充气轮胎的方法，包括以下步骤：混合包含弹性体、填料、稀释剂、醌型固化剂、氧化剂型共固化剂；和式1的固化活化剂的密封剂组合物：
其中R1和R2独立地为H或C1 至C4烷基，或者R1 和R2连接在一起形成取代或未取代的亚苯基基团；R3 和R4 独立地为H、-OH、-NH2、C1 至C4烷基或-OR5，其中R5为C1 至C4烷基，条件是当R1 和R2连接在一起形成取代或未取代的亚苯基基团时，R5为C1 至C3烷基；将该密封剂组合物施加到固化轮胎的内表面上；并固化该密封剂组合物。
在图1中，呈现了固化充气轮胎10的横截面，所述固化充气轮胎10包括胎面14（其包括胎面基部橡胶层11）、侧壁12、间隔开的胎圈18和胎面14（包括胎面基部层11）下方的胎体，其包括帘线增强（例如钢丝帘线增强）的橡胶带束帘布层16、帘线增强（例如合成尼龙或聚酯帘线增强）的橡胶胎体帘布层17和任选的橡胶阻挡层13，其中内衬橡胶层22定位在胎体的径向内侧并且任选的阻挡层13和胎体帘布层17与密封剂层20一起形成轮胎的径向最内表面。
密封剂层由具有表1中所示的一般组分的组合物形成。
表1
合适的式1的固化活化剂包括邻苯二甲酸、邻苯二甲酸单烷基酯、邻苯二甲酸二烷基酯，如邻苯二甲酸二甲酯、邻苯二甲酸二乙酯和邻苯二甲酸二丙酯，邻苯二甲酸单酰胺、邻苯二甲酸二酰胺、邻苯二甲醛和邻二乙酰苯；马来酸、马来酸单烷基酯、马来酸二烷基酯，如马来酸二甲酯、马来酸二乙酯、马来酸二丙酯和马来酸二丁酯，马来酸单酰胺、马来酸二酰胺、柠康酸、柠康酸单烷基酯、柠康酸二烷基酯、柠康酸单酰胺、柠康酸二酰胺和2-丁烯二醛-2Z；偏苯三甲酸、偏苯三甲酸单烷基酯、偏苯三甲酸二烷基酯、偏苯三甲酸三烷基酯、连苯三甲酸、连苯三甲酸单烷基酯、连苯三甲酸二烷基酯、连苯三甲酸三烷基酯、均苯四甲酸、均苯四甲酸单烷基酯、均苯四甲酸二烷基酯、均苯四甲酸三烷基酯和均苯四甲酸四烷基酯。
密封剂层包含弹性体。合适的弹性体包括异戊二烯-异丁烯-橡胶（丁基橡胶，IIR）、卤化异戊二烯-异丁烯-橡胶（HIIR）、乙烯-丙烯-二烯-三元共聚物（EPDM）、苯乙烯-丁二烯共聚物（SBR）、丙烯腈-丁二烯共聚物（AB）、丙烯腈-丁二烯-苯乙烯共聚物（ABS）、聚丁二烯、天然橡胶、顺式聚异戊二烯、及其组合。合适的弹性体通常具有100 kDa至500 kDa的分子量Mn。分子量Mn可以通过本领域中已知的方法（例如通过按照ASTM D3536或等同物的凝胶渗透色谱法）测定。
在一个实施方案中，密封剂层包含丁基橡胶。如本文中所用的术语“丁基橡胶”定义为表示主要由异丁烯的重复单元组成但包含少量共轭二烯的重复单元的聚合物。优选丁基橡胶的约85重量％至约99.5重量％是衍生自异丁烯聚合的重复单元，而约0.1重量％至约15重量％的重复单元衍生自具有4至8个碳原子的共轭二烯，如丁二烯、异戊二烯、己二烯等，其中优选异戊二烯。
密封剂层还包含稀释剂。合适的稀释剂包括数均分子量Mn为200至5,000的低分子量弹性体。低分子量弹性体包括低分子量聚异戊二烯、聚丁烯（包括聚异丁烯）、聚丁二烯、丁基橡胶等。其它稀释剂包括油和树脂。分子量Mn可以通过本领域中已知的方法（例如通过按照ASTM D3536或等同物的凝胶渗透色谱法）测定。
在一个实施方案中，稀释剂是聚丁烯。聚丁烯是指一种或多种丁烯异构体（包括1-丁烯、2-丁烯和2-甲基丙烯（异丁烯））的聚合物。这样的聚丁烯在商业上可称为聚异丁烯。
此类聚丁烯优选具有超过约600的数均分子量，以尽量减小从密封剂层迁移到邻近轮胎组件中的可能性。其优选通过用金属卤化物催化剂使富含异丁烯的物流聚合而制备，并且优选具有类似聚异丁烯的聚合物骨架结构。非常合适的聚丁烯可以以商标Indopol获得。在一个实施方案中，聚丁烯的数均分子量（Mn）为约600至约2500，如通过蒸气压渗透压力测定法测定的那样。
油可以作为稀释剂包含在密封剂中。合适的油包括诸如以下的油：矿物油，包括但不限于芳烃油、环烷油、石蜡油、MES油、TDAE油、RAE油和SRAE油，以及植物油，包括但不限于向日葵油、大豆油、玉米油、蓖麻油和低芥酸菜子油。油可以以5至15 phr的量存在。
树脂也可以作为稀释剂包含在密封剂中。合适的树脂包括烃树脂、酚/乙炔树脂、松香衍生的树脂及其混合物。代表性的烃树脂包括香豆酮-茚-树脂、石油树脂、萜烯聚合物及其混合物。
密封剂中弹性体成分的交联可以通过已知的醌型体系之一来实现。在醌型固化体系中，苯醌二肟和对对二苯甲酰醌二肟优选作为固化剂。其它合适的固化剂包括二苯甲酰对醌二肟、对二亚硝基苯和N-甲基-N,4-二亚硝基苯胺。可用于密封剂组合物中的交联活化剂包括有机过氧化物（包括二芳酰基过氧化物、二酰基过氧化物和过氧化酯。在一个实施方案中，固化剂/交联活化剂组合是苯醌二肟和过氧化苯甲酰组合。
其它常规配混成分可包括在混合过程中，包括但不限于填料，如炭黑和二氧化硅、抗降解剂、着色剂、加工助剂等。
除式1的固化促进剂外，密封剂组合物还可包含选自乙二醇、烷基取代的乙二醇、乙二胺和烷基取代的乙二胺的固化迟延剂。合适的固化迟延剂包括乙二醇、丙二醇（即α-丙二醇）、乙二胺、甲基乙二胺、N,N-二甲基乙二胺和1,2-二甲基乙二胺。固化迟延剂的使用量范围可以与固化促进剂相同。
密封剂组合物的混合可以例如通过在橡胶混合机，如Brabender密炼机、挤出机、锥形混合机等中组合弹性体和其它组分来实现。用于混合密封剂和施加至轮胎内衬的合适方法如例如公开在US 8,821,982中。
在混合和固化之后，将密封剂组合物施加到固化轮胎的内衬上。在施加密封剂之前，可以清洁轮胎内衬的表面杂质，以改善密封剂对内衬表面的粘附性。在一个实施方案中，使用如US 2017/0151740中所述的激光技术清洁内衬表面。
图2描绘了硫磺固化充气轮胎10的局部横截面（在图2中标记为10a），包括具有其胎面基部橡胶层11的轮胎胎面14、钢丝帘线增强的橡胶带束帘布层16、胎体，其具有合成帘线增强的橡胶胎体帘布层17（例如基于合成纤维的帘线，例如尼龙或聚酯帘线）、任选的橡胶阻挡层13、橡胶内衬22和密封剂层20。密封剂层20施加到已经固化的轮胎的内衬22上（因此是轮胎固化后施加的密封剂层）以为轮胎提供具有针对各种刺穿物体的防刺穿性能的密封剂层。
周向密封剂层20的厚度可以在一定程度上根据所需的密封能力的程度以及轮胎本身（包括轮胎尺寸和预期轮胎用途）而改变。例如，密封剂层的厚度可以为约0.13厘米（0.05英寸）至约1.9厘米（0.75英寸），这在一定程度上取决于轮胎本身及其预期用途。例如，在乘用车轮胎中，密封剂层20可以例如具有在约0.33厘米（0.125英寸）范围内的厚度，而对于卡车轮胎，密封剂层20可以例如具有在约0.76厘米（0.3英寸）范围内的厚度。轮胎固化后施加的密封剂层20通常位于轮胎10的胎冠区域中，并且如果需要的话，其可以包含着色剂，使得其具有非黑色，这可以与黑色内衬、胎面或侧壁形成对比，以便可以注意到轮胎刺穿。
轮胎内衬橡胶层22可以包括用于充气轮胎的常规硫磺固化型橡胶内衬。在一个实例中，橡胶内衬22可以是卤代丁基橡胶（例如氯丁基橡胶或溴丁基橡胶）的含硫磺固化剂的卤代丁基橡胶组合物。这种基于卤代丁基橡胶的内衬层还可含有一种或多种硫磺固化型基于二烯的弹性体，例如顺式-1,4-聚异戊二烯天然橡胶、顺式-1,4-聚丁二烯橡胶和苯乙烯/丁二烯橡胶或其混合物。内衬22通常通过常规的压延或研磨技术制备，以形成适当宽度的未固化配混橡胶条。当轮胎10固化时，内衬22发生共固化，由此与轮胎10成一体。轮胎内衬橡胶层及其制备方法是本领域技术人员所熟知的。
实施例1
在本实施例中，举例说明了几种固化改性剂对轮胎密封剂组合物的固化的影响。使用表2中所示的量在实验室混合机中混合四种密封剂组合物，其量以重量百分比给出。测试混合样品的固化特性，包括最小扭矩和最大扭矩（Smin、Smax）、Δ扭矩（Smax-Smin）和T点，结果在表3和图3中给出。这样的“T点”（即T90 、T25、T80等）代表硫化状态，其对于本领域技术人员而言是可认识的并且在ASTM D2084、D5289和ISO 6502中定义，并且充分描述在1990年11月5-6日H. G. Buhrin于Brighton, England在Tyretech '90给出的报告中。使用Flexsys橡胶加工分析仪（RPA）2000测定扭矩和T点。在这些参考文献中可以找到RPA 2000的说明、其性能、样品制备、测试和子测试： H A Pawlowski和J S Dick，Rubber World，1992年6月；J S Dick和H A Pawlowski，Rubber World，1997年1月；以及J S Dick和J APawlowski，Rubber & Plastics News，1993年4月26日和5月10日。
如图3中所示，与对照（1）相比，添加邻苯二甲酸二甲酯（3）或马来酸二丁酯（2）显示出密封剂固化的增强。添加乙二醇（4）显示出对固化的抑制作用。
表2
1 来自ExxonMobil的Butyl 269
2 来自Cabot的Vulcan M
3 Indopol H300
4 Luxomaxx K-CDO
5 法兰西提锌法
6 来自Pergan的Peroxan BP50 PF1，50重量%的过氧化二苯甲酰。
表3

Claims (10)

1.制造充气轮胎的方法，其特征在于包括以下步骤：
混合包含弹性体、填料、稀释剂、醌型固化剂、氧化剂型共固化剂；和式1的固化改性剂的密封剂组合物：
其中R1和R2独立地为H或C1 至C4烷基，或者R1 和R2连接在一起形成取代或未取代的亚苯基基团；R3 和R4 独立地为H、-OH、-NH2、C1 至C4烷基或-OR5，其中R5为C1 至C4烷基，条件是当R1 和R2连接在一起形成取代或未取代的亚苯基基团时，R5为C1 至C3烷基；将所述密封剂组合物施加到固化轮胎的内表面上；并固化所述密封剂组合物。
2.权利要求1的方法，其特征在于所述固化改性剂选自邻苯二甲酸、邻苯二甲酸单烷基酯、邻苯二甲酸二烷基酯、邻苯二甲酸单酰胺、邻苯二甲酸二酰胺、邻苯二甲醛和邻二乙酰苯；或者所述固化改性剂选自马来酸、马来酸单烷基酯、马来酸二烷基酯、马来酸单酰胺、马来酸二酰胺、柠康酸、柠康酸单烷基酯、柠康酸二烷基酯、柠康酸单酰胺、柠康酸二酰胺和2-丁烯二醛-2Z；或者所述固化改性剂选自偏苯三甲酸、偏苯三甲酸单烷基酯、偏苯三甲酸二烷基酯、偏苯三甲酸三烷基酯、连苯三甲酸、连苯三甲酸单烷基酯、连苯三甲酸二烷基酯、连苯三甲酸三烷基酯、均苯四甲酸、均苯四甲酸单烷基酯、均苯四甲酸二烷基酯、均苯四甲酸三烷基酯和均苯四甲酸四烷基酯。
3.权利要求1的方法，其特征在于所述密封剂组合物进一步包含选自乙二醇、烷基取代的乙二醇、乙二胺和烷基取代的乙二胺的固化迟延剂。
4.权利要求1的方法，其特征在于所述弹性体选自丁基橡胶、卤化丁基橡胶、EPDM、苯乙烯-丁二烯橡胶、丙烯腈-丁二烯橡胶、丙烯腈-丁二烯-苯乙烯橡胶、聚丁二烯、天然橡胶和合成聚异戊二烯。
5.权利要求1的方法，其特征在于所述氧化剂型共固化剂选自二芳酰基过氧化物、二酰基过氧化物和过氧化酯。
6.权利要求1的方法，其特征在于所述醌型选自苯醌二肟、对对二苯甲酰醌二肟和二苯甲酰对醌二肟。
7.权利要求1的方法，其特征在于所述稀释剂是数均分子量Mn为200至5,000的低分子量弹性体。
8.权利要求1的方法，其特征在于所述密封剂组合物进一步包含1至10 phr的金属氧化物，所述金属氧化物选自氧化锌、氧化镁和氧化钙。
9.权利要求1的方法，其特征在于混合的步骤包括以下步骤：
将氧化剂型共固化剂与一部分稀释剂组合以形成组分A；
将剩余的成分组合以形成组分B；和
将组分A与组分B混合以形成所述密封剂组合物。
10.充气轮胎，其特征在于通过权利要求1的方法制造。
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EP3572218A1 (en) 2019-11-27
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